Conversion of cellular or fibrous material



June 29 1926. 1,590,593

E. TAYLOR ET AL CONVERSION OF dELLULAR on FIBROUS MATERIAL Filed Dec. 2, 1919 a lNVENTOR [H BY I ATTORNEY Patented June 29, 1926.-

"UNITED STATES PATENT orrlca.

EDWIN TAYLOR AND EDWARD F. CHANDLER, OF BROOKLYN, NEW

YORK, Assmnons,

BY MESNE ASSIGNMENTS, TO TAYLOR LABORATORIES-INQ, NEW YORK, N. Y., A

CORPORATION OF NEW YORK.

CONVERSION OF CELLULAR OR FIBBOUS MATERIAL.

Application filed December 2, 1919. Serial No. 341,853.

The invention relates to improvements in the conversion of cellulose or fibrous matev such as cel rial. In our prior co-pending application may be so treated more expe itiously and in a more economical and useful manner. Further and more specific objects, features and advantages will more clearly appear from the detail description given below.

In the preferred method of practicing the inventive .idea the organic or cellulose material to be converted is dissolved preferably in an excess of cupro-ammonia solution, filtered to remove extraneous impurities, the solution concentrated by the partial removal of ammonia and water (as for instance by means of a vacuum), the resulting homogeneous fluid flowed on a carrier which may be a. flexible band of metal suitable for employment as one of the elements of an electrolytic cell, the said carrier being adapted to convey the flowed material through preferabl a dry and inert gas, thereby excluding eleterious atmospheric contamination.

The carrier conveying the flowed material now enters and becomes preferably one of the elements or electrodes, in a bath which may' be provided with another element or 'electrode so as to constitute an electrolytic cell upon the energization of the said elements and through which the carrier which may be the anode, is adapted to continuously convev the flowed material. Owing to the electrolytic characteristics of cellulose anic matter;

' resistance to moisture.

pleted under proper conditions of time and current density before the carrier and material leaves the. cell. During the eriod of transformation the volatile constituent is released from the mass and is in a condition to be conveyed to a suitable condensing or'recovering system, the metallic constituent being deposited on the cathode in recoverable condition. ganic material free of all traces'of anyingredient that might cause future deterioration is preferably conveyed throu h a suitablewashing system where any a ering or extraneous traces of foreign materials are removed and thence to a suitable drying system for the removal of any moisture content after which the converted material is ready for separationv from the conveyor or carrier.- This separationmay be elfected'by means of a V-shaped fixed edge supplemented by two rolls.

The transformed or-' The material, now in a transparent flexible band resembling celluloid in appearance is then led through a bath containing a volatile solvent such as amyl-acetate which possesses a slight solvent or softening effect on the cellulose and materially aids in increasing its surface lustre, its density, and its The material still wet with solvent is now passed through warm calender rolls whereon it is surfaced, brought to exact thickness and dried and the solvent recovered. From the calenders the finished product may be wound on reels, cut or trimmed in sheets or strips or other- ,wise dis osed of.-

It wil be seen that this process is eco-. nomical, as well as continuous. All the solvent materials are recovered in usable form fromfor resolution, even the trimmin the finished material being returns to the solution tanks. The power factor is low and the amount of labor re 'uired is almost negligible. It is evident t at the above process can be advantageously carried out by the use of a concentrated zinc chloride solution, etc., in place of the cupro-amin a colloidal state, the flowed materialas it ,monia.

passes through the infiuence'of the saidelec tric field or fields is converted from the colloidal solution to a solid or more dense state which transformation should be com- In the accompanying drawings we have illustrated a suitable application of our invention as applied to the manufacturin of photographic films. In said drawings, ig.

till

"down through the chamber 18, it passes be cross-sectional detail of the endless belt and film formed thereon.

3-4 indicate suitable tanks carrying concentrated solution of 'cupro-aminonia or concentrated solution of Zinc chloride both being good solvents for cotton which may be used in the manufacturing or" the film. About one pound of cotton may be used to about twenty pounds of the solution and suitable means such as the valve 5 may be provided "for regulating the How of the material upon the endless belt 6 which passes entirely through the closed tray or chamber 7 as shown.

The belt may be made of copper and may be plated with other metal and buffed and may besuitably perforated as indicated at 8 in Fig. 2 to receive the teeth of sprocket wheels for driving the same, suitable means for driving the belt being provided such as 9, an electric motor connected to the driving shaft 10. Upon the belt may be provided suitable strips of material such as 11 between which the flowing material from the tanks 3 l is deposited. lln the drawing 1 have illustrated the belt as traveling from left to right looking at Fig. l.

The ammonia from the closed tray 7 is drawn through the outlet pipe 12 by the suctan 1% and is passed. through the drying chamber i l provided with suitable grids 15 upon which lime or other suitable .material 15' may be piled, the dry ammonia returning through the pipe 16 into the closed tray 7 as shown. This provides a constant circulation of dry ammonia gas in the closed chamber and prevents waste of material and contamination from the outside.

17' indicates an electrolytic cell to be hereafter more fully referred to and is in communication with the superimposed chamber ,18 through which ammonia, hydrogen, oxygen or other gases rise and escape by way of the pipe 19 controlled by the valve 20 into the chamber 21 escaping under the hood 22 for condensation and recovery except when the valve 23 is open to allow the same to pass to the drying chamber 14.

The electrolytic bath 17 may be provided with copper electrodes 24; or when the process is worked. with zinc chloride, zinc electrodes may be used. An acidulated solution of nitric or sulphuric acid 25 is provided as an electrolyte sufiiciently strong to carry the current.

As the cellulose fed upon the belt 6 passes noath the first electrode 24 at the right side oi the figure over the pulley 26, beneath the next electrode. over the next pulley and so on until it enters the chamber 27, said pub menses leys being driven by the worms 28 upon the motor shaft 10 and said electrodes being connected to the negative side of a suitable source of electricity as shown, with the result that the metallic content of the cellulose upon the belt is electrodeposited therefrom upon the electrodes 24 leaving the cellulose gradually becoming white instead of blue or green as it passes through the electrolytic bath until upon leaving said bath the cellulose is quite white. whereupon it enters the washing tank 27 before referred to. The film is now sutficiently tough and flexible for Washing whereas if the metallic content remained in the film, it would upon drying be brittle and liable to breakup. In the washing tank 27 water enters by the pipe 29 con-. trolled by the valve 30 and escapes by the pipe 81 which may be provided with a valve 82, the film passing over the pulleys driven by the worms 3% upon the said motor shaft 10, and a suitable partition may be provided with an opening at the bottom as indicated at 86 so as bring the film in contact with th cleaner water of the wash as it leaves the tank 27. All of these tanks are preferably closed to prcvent'foreign matter from coming in Contact with the film and if desired suitable means may be provided for evacuating air therefrom as any carbonic acid present in the room is apt to form carbonate, this especially applies to the drying tank and various other objectionable results may be encountered. The washing tank removes any adhering ammonia, acid, of particles of matter, after which the film passes to the drying chamber 37 Where it again passes over pulleys such as 38 driven by worms such 39 and beneath pulleys such as 40 until it finally emerges over the pulley ell as shown. lhis drying tank may of course be heated by any suitable means to a temperature. say perhaps 120- degrees Fahrenhcit. The film is now loosened from the belt upon which it was formed and due to the heat, shrinkage, etc., is readily separated therefrom, and in this connection suitable knife or stripper such as 42 may be provided adjacent the periphery of the roll 41 so as to allow the film to pass leitwardly between the rollers 3 of the tank 44 while the belt or carrier passes downwardly beneath the pulleys from which point it returns to the starting place and again passes through the closed tray 7.

The detached film upon entering the tank ll passes over th roller lt? driven by the worm 47 and downwardly through. the ainyl acetate bath 48 passing upwardly again over the roller 19 and upon the rolls 50 preferably of highly polished surface. In the amyl acetate tank the film is softened, densified, and is increased in its resistance to moisture, after which, upon passingfirst leitw rdly around the top roll 50, then rightwardy lid menses roll below, leftwardly combustible and of numerous other properties and advantages.

ie of the advantages in the use of our for photographic purposes is that it be impregnated from one side (preferably unealendered) with a solution of silver salt, such as nitrate ofsilver, after which the film may be exposed to an atmosphere of, and impregnated with bromine, chlorine, iodine or a combination thereof, thereby depositing insoluble bromide or chloride etc. of silver in the film itself. It will be found er that after the same has been photoanically exposed and developed there is no uniting oil or scratching oft of the negative surface, thus preventing the objection effects in photography so much complained of, as even if the surface of our film he sci "lied er mutilated, the cl emicals hay penetrated the film, still present the photographic image, which in the path of the light registers the characters, notwithstanding the mutilated surface of the film.

Another advantage of our process resides the fact that by passing the film from the drying chamber 37 through any well irnown form of nitrate bath of any desired consistency, a pyroxyline may be obtained in a dense continuous sheet haying the same nitrogen content as the original cotton immersed under equal conditions in the same This provides ,a ready means for btlmi, manufacturing granulated smokeless powder without the use of a volatile solvent.

The cupro-ammonia solution he'reinbefore referred to is preferably made by dissolving vdrated cupric-oxide Gui-LO, in approxima ely an equal weight of ammonia water containing; thirty per cent (30%) ammonia hydrate NELOH. The resulting solution is of an intensely blue color and may be considered to be merely a mixture of cupricoxide, (CuO) ammonia (NH,) and water.

We have found even under adverse conditions that with about two amperes per square inch of anode, that we can obtain about forty grams of cellulose and about twentythree and one-half grams of copper in about an hour and a half. This however is not so on alternately, it becomes,

2 by preparing photographic films in this submitted. an. accurate statement as what may be done under more favorable conditions.

0f course it will be understood that changes clients and proportions thereof and in the manner of manipulating the same without departing from the spirit of the invention as claimed.

We claim:

1. A method of dissolving organic material while in a cellular or fibrous condition or which has been in such condition, in a solvent containing a plurality of combined chemical elements, at least one of said elements being a .metal, and at least one being volatile, passing the resultant colloidal solution through an electrolytic field or fields thereby causing the metallic constituent to be electrolytically extracted and deposited upon one electrode, the volatile constituent to be released from solution, and the organic material to be deposited on the other electrode in a homogeneous condition without change in its original chemical constitution.

2. A method of dissolving organic material while in a cellular or fibrous condition or which has been in such condition, in a solvent containing a plurality of combined chemical elements, at least one of said elements being a metal, and at least one being volatile, passing the resultant colloidal solution through an electrolytic field or fields thereby causing the metallic constituent to be electrolytically eritracted and deposited upon one electrode, the volatile constituent to be releasedfrom solution, and the organic material to be deposited on the other electrode in a homogeneous condition without change in its original chemical constitution, and providing means for recovering both metallic and volatile constituents and returning them together with successive portions or quantities of organic material to the electric field. i

3. A method of dissolving organic material and placing same in solution on a moving carrier, causing said material to deposit as a. homogeneous solid on the carrier by means of an electric current, removing the solid material from the carrier and improving its physical character by means of volatile solvents combined with mechanical pres-- sure.

4. A method of dissolving cellular or fibrous organic material in a solvent containing a plurality of chemical elements, at least one of said elements bein a gas, placing the solution on a continudusly moving carrier surrounded by a moving atmosphere of the said'gas in a dry condition thereby tending to concentrate the solution of organic material and preventing access of external deleterious gases or substances, allowing the organic material to remain in this may be made in the various ingre- Ill? - the material continuously through the &

atmosphere until it is in a homogeneous state returning the gas to its source of supply andv removing the homogenous material.

5. The method of producing cellulose whichconsists in dissolving organic matter in a suitable solvent, flowing the solvent carrying the dissolved organic matter into a sheet or film and then subjecting the sheet or film to electrical action.

6. In an apparatus of the class described, an endless conveyor, a chamber through which said conveyor serving as an electrode travels through which material may be fed upon said conveyer to form a film, means for passing said film through an electrolyte provided with electrodes, means for extracting the metallic content of said film through said electrolyte, means for thereafter washing said film, means for thereafter drying said film, means for thereafter finally separating and treating said film.

7, In an apparatus of the class described, an endless conveyer, a chamber through which said conveyer serving as an electrode travels through which material may be fed upon said conveyor to form a film, means for passing said film through an electrolyte provided with electrodes, means for extracting the metallic content of said film through said electrolyte, means for thereafter washing said film, means for thereafter drying said film, means for thereafter finally separating and treating said film, and in combination, means for recovering the materials used in the treatment oi said film.

8. The method or treating cellulose material which consists in providing an anode carrier, in an electrolytic cell with a solution of the cellulose material between the cathode of the cell and said anode carrier, and passing a direct current through the cell rom one of said electrodes to the other, and finally stripping the cellulose from the anode carrier.

9. The method of treating cellulose material which consists in passing an anode car- 'rier through an electrolyte in an electrolytic cell, and electrolyzing the cellulose on said carrier as it passes through the electrolyte.

10. The method of treating organic material which consists in passing a carrier J. the material continuously through the trolyte-of an electrolytic cell, and ele lyzing the organic material on the on as it passes through the electrolyte.

11.. The method of treating cellulosic terial which consists in passing a carrier trolyte of an electrolytic cell, electroly the cellulose on the carrier as it passes through the cell, and without stopping passing the electrolyzed cellulose through a washing bath,

12. The method of treating organic n1atcrial which consists in passing a carrier for incomes paratus consecutively.

14. The method of treating cellulosic material which consists in placing a layer of the cellulosic material on a carrier, and moving the carrier through the electrolyte of an electrolytic cell, electrolyzing the cellulose on said carrier as it passes through the electrol te."

15. he method of treating cellulose material which consists in passing an anode carrier through an electrolyte in an electrolytic cell, electrolyzing the cellulose on said carricr as it passes throu h the electrolyte while maintaining the cell closed to the outside atmosphere.

16. The method of treating cellulose material which consists in passing an anode carrier through an electrolyte in an electrolytic cell, electroly'zing the cellulose on said carrier as it passes through the electrolyte, and Without stopping assing the treated cellulose through a wasliing bath and drying apparatus consecutively, the cellulose being kept substantially free of CO while passing throu h the electrolytic cell, wash ing bat and .rying apparatus.

17. The method of treating cellulosic material which consists in placing a layer of the cellulosic material on a carrier, and moving the carrier through the electrolyte of an electrolytic cell, electrolyzing the cellulose on said carrier as it passes through the elec trolyte, and keeping the cellulosic material substantially free of CO of the air after it is placed on said carrier and until it has left said cell,

18. The method of treating cellulose which consists in preparing a solution of cellulosic material, placing same on a moving carrier in an atmosphere of an inert gas, and passthe carrier through an electrolyte, electrolyzing the cellulose on the carrier.

9. The method 1 of treating cellulose h consists in preparing a.solution of losic material, placing same on a movcarrier in an atmosphere of an inert gas, i passing the carrier through an electrolyte, electrolyzing the cellulose on the carrier, said electrolyte being in a cell closed to the outside atmosphere.

The method which consists in passing electrode carrier through an electrolytic teriocl which consists preparing a this:

cell and 'leriul sols: W solution elect lyri ally and cellulose riecl from the cell on the carrier.

21. The method of treating cellulosic masolution thereof, applying a layer of the so;-

lution to endless bend passing ud hand through en el ctrolytic cell in Wh 1?:

forms the anode, thcrehy elem-rolyzing the cellulose on said band.

The method of treating organic material which consists in applying e thick solution of organic meteri to a moving carrier, and p "sing "the sen i the our throu ictrolyte in ectrclytic the soiution on c i the concentrated rier and the so through an electrolyte in an electrolytic cell on the "lulosic me solution electrolyzing the solution on the carrier and d positing the metal of the so t on a cathode the electrolytic hath, the carrier forming an suede on which the cellulose is electrolyzedr :25. The method of treating cellulosic material which consists in preparing a solution of the cellulosic material passing a, carrier through an electrolytic cell and electrolyzing the cellulose on the carrier as it passes through the electrolytic cell.

26. The method of treating celluosic mi,- teriel which consists in subjecting the same to electrolysis to deposit the cellulose electrolytically and treating cellulose with a, volatile organic softening agent.

27. The method of treating cellulosic mawhich consists in subjecting the same trolysis to deposit the cellulose elecicelly and treating cellulose with amyl acetate, l

28. The method of treating cellulosic material which consists in preparing a solution or? the cellulosic material, applylng said solution to a moving carrier, moving the solution on said carrier through an atmosphere of ammonia into an electrolytic bath and electrolyzing the cellulose 0n the carrier therein.

In testimony whereof We hereunto eifix our signatures.

EDWIN TAYLOR. EDWARD F. CHANDLER. 

